CN109585839A - A kind of alumina-coated nickel-cobalt-manganternary ternary anode material and its preparation method and application - Google Patents
A kind of alumina-coated nickel-cobalt-manganternary ternary anode material and its preparation method and application Download PDFInfo
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
The invention discloses a kind of alumina-coated nickel-cobalt-manganternary ternary anode material and its preparation method and application, material the preparation method is as follows: instill aluminum nitrate in (1) ammonium hydroxide, citric acid and nitric acid are added when reaction is not further added by sediment, prepares AlOOH colloidal sol；(2) nickel cobalt manganese presoma and lithium source are uniformly mixed, nickel-cobalt-manganese ternary material is obtained after sintering；(3) nickel-cobalt-manganese ternary material is placed in AlOOH colloidal sol, is calcined after dry, finally obtains alumina-coated nickel-cobalt-manganternary ternary anode material.By coating one layer of alumina-coated layer in nickel-cobalt-manganese ternary material surface, the residual alkali amount of material surface is reduced, effectively inhibits the side reaction between material and electrolyte, improves the security performance of battery；In addition, thus battery made of material, alumina-coated layer can form Li-Al-Co-O protective layer on the surface of the material at work, which can resist corrosion of the HF to active material, improve the cycle performance of battery.
Description
Technical field
The present invention relates to field of lithium ion battery anode, specifically a kind of alumina-coated nickel-cobalt-manganese ternary anode material
Material and its preparation method and application.
Background technique
With the aggravation of environmental pollution and gradually using up for fossil energy, environmentally protective new-type energy is found as various countries
The main problem faced；Lithium ion battery has energy density compared to traditional lead-acid battery, nickel-cadmium cell and nickel-metal hydride battery
It is high, have extended cycle life, the advantages that charge and discharge voltage is high, environmentally protective, memoryless, just obtained since the birth eighties in last century
Fast development, at present the battery not only has been widely used on the electronic products such as 3C, even more becomes new-energy automobile
The first choice of power battery becomes the emphasis of various countries' research.
Lithium ion battery composition part mainly includes the several majors such as positive electrode, negative electrode material, diaphragm, electrolyte,
Middle positive electrode occupies 30% or more of battery cost, even more decides the performance of battery, becomes the weight of Study on Li-ion batteries
Point.Currently, popular positive electrode mainly has LiCoO in the market2、 LiFePO4With Li [Ni, Co, Mn] O2Material.
Li[Ni,Co,Mn]O2Series material abbreviation ternary material, it combines LiCoO2Good circulation performance, LiNiO2
Height ratio capacity and LiMnO2High safety performance and low cost etc., become after LiFePO4And LiCoO2Another mainstream anode afterwards
Material；Now with the continuous improvement that new-energy automobile requires battery energy density, nickelic ternary material becomes the heat of research
Point, but with the raising of nickel content, a series of problem can also occur, such as: cycle performance is deteriorated, and surface residual alkali increases,
Phenomena such as thermal stability is deteriorated, and surface reaction is uneven, hinders its application in power battery.
Summary of the invention
The purpose of the present invention is to provide a kind of alumina-coated nickel-cobalt-manganternary ternary anode material and preparation method thereof and answer
With to solve the problems mentioned in the above background technology.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of alumina-coated nickel-cobalt-manganternary ternary anode material, specifically includes the following steps:
(1) ammonium hydroxide is added in a reservoir, is placed in heating stirring in water-bath, instills aluminum nitrate solution and generates sediment, reacts to heavy
When starch is not further added by, citric acid and nitric acid is added, hydrolyzes sediment, peptization obtains AlOOH colloidal sol after aging；
(2) nickel cobalt manganese presoma and lithium source ball milling mixing is uniform, nickel-cobalt-manganese ternary material is obtained after oversintering；
(3) nickel-cobalt-manganese ternary material is placed in AlOOH colloidal sol, continues agitating and heating, is calcined after evaporation drying,
Finally obtain alumina-coated nickel-cobalt-manganternary ternary anode material.
The concentration of ammonium hydroxide is 0.5-2mol/L in the step (1) as a preferred technical solution, and the temperature of water-bath is
80-100 DEG C, the concentration of aluminum nitrate solution is 0.2-0.6mol/L, and the concentration of nitric acid is 0.5-1mol/L；Citric acid and aluminum nitrate
The molar ratio of aluminum nitrate is 1:1 in solution.
The time of aging is 10-20h in the step (1) as a preferred technical solution,.
As a preferred technical solution, in the step (2) lithium source be selected from the oxide of lithium, hydroxide, carbonate,
At least one of acetate, oxalates.
The molar ratio of nickel cobalt manganese presoma and lithium source is 1:(1.02- in the step (2) as a preferred technical solution,
1.07),
Further, the chemical general formula of the nickel cobalt manganese presoma is NiaCobMnc(OH)2, wherein 0.6≤a≤0.8,0.1≤b
≤ 0.20,0.1≤c≤0.2.
The specific steps being sintered in the step (2) as a preferred technical solution, are as follows: with heating rate 5 DEG C/min liter
Temperature keeps the temperature 3-5h to 500-550 DEG C, then proceedes to be warming up to 800-870 DEG C, keeps the temperature 10-15h；The atmosphere of sintering is oxygen, sky
One of gas, compressed air；The gas flow of sintering is 0.5-1.5L/min.
Nickel-cobalt-manganese ternary material and the molar ratio of AlOOH colloidal sol are in the step (3) as a preferred technical solution,
1:(0.002-0.006).
The heating rate calcined in the step (3) as a preferred technical solution, is 5 DEG C/min, and the temperature of calcining is
600-750 DEG C, the time of calcining is 5-10h.
It is a further object to provide alumina-coated nickel-cobalt-manganese ternary anodes prepared by the above method
Material.
Third object of the present invention is to provide above-mentioned alumina-coated nickel-cobalt-manganternary ternary anode materials to prepare lithium ion
Application in battery.A kind of lithium ion battery, lithium ion battery include shell and be placed in the intracorporal anode of shell, cathode, diaphragm and
Electrolyte, diaphragm are located between the anode and cathode, and diaphragm is gluing ceramic diaphragm, and cathode is artificial graphite, and electrolyte is
The LiPF of 1.0mol/L6The electrolyte of/EC+EMC+DEC, shell are rectangular aluminum hull, the just extremely alumina-coated nickel cobalt manganese
Tertiary cathode material.
Compared with prior art, the beneficial effects of the present invention are:
(1) alumina-coated nickel-cobalt-manganternary ternary anode material of the invention have high circulation performance and high safety performance, by
Nickel-cobalt-manganese ternary material surface coats one layer of alumina-coated layer, reduces the residual alkali amount of material surface, effectively inhibits material
Side reaction between electrolyte makes battery produce gas in cyclic process less, effectively increases the security performance of battery；In addition,
Thus battery made of material, alumina-coated layer can form Li-Al-Co-O protective layer, the guarantor on the surface of the material at work
Sheath can resist corrosion of the HF to active material, effectively prevent the dissolution of metal ion in the electrolytic solution in material, improve
The structural stability of material under high voltages, improves the cycle performance of battery.Moreover, the presence of the protective layer can also drop
The surface impedance of low material improves the high rate performance of material.
(2) this method carries out surface packet by first synthesizing AlOOH colloidal sol, then to the nickel-cobalt-manganese ternary material synthesized
Cover, method is simple and effective, so that the material surface finally obtained is uniformly coated one layer of alumina-coated layer, the lithium comprising this material from
Sub- battery has better cycle performance and security performance.
(3) present invention, can be in nickel cobalt after calcining by mixing nickel-cobalt-manganese ternary material with AlOOH colloidal sol
One layer of alumina-coated layer of manganese ternary material coated with uniform, and alumina-coated layer particle is tiny, and specific surface area is larger,
Covered effect is more preferable, is easier to form one layer of fine and close protective film on ternary material surface.
Detailed description of the invention
Fig. 1 is the XRD diagram of alumina-coated nickel-cobalt-manganternary ternary anode material prepared by embodiment 1；
Fig. 2 is the SEM figure of alumina-coated nickel-cobalt-manganternary ternary anode material prepared by embodiment 2；
Fig. 3 is the high-temperature expansion rate figure of battery prepared by embodiment 3；
Fig. 4 is the normal-temperature circulating performance figure of battery prepared by embodiment 3.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Test method described in following embodiments is unless otherwise specified conventional method；The reagent is such as without special theory
It is bright to be obtained through commercial channels.
Embodiment 1
(1) ammonium hydroxide of 1mol/L is added in a reservoir, is placed in laser heating in 80 DEG C of water-baths and stirs, be then slowly dropped into
0.2mol/L aluminum nitrate solution, generates sediment slowly；It reacts to sediment not when increasing, then citric acid is added thereto
With 0.5mol/L nitric acid solution, hydrolyze sediment slowly, peptization continues to obtain clear AlOOH after stirring aging 10-20h
Colloidal sol；
(2) in molar ratio 1:1.06 by presoma Ni0.6Co0.2Mn0.2(OH)2With LITHIUM BATTERY LiOHH2O mixes ball together
Mill, it is to be mixed to be uniformly placed in alumina ceramic crucible, it is sintered in the case where being connected with compressed air, wherein be sintered
Gas flow is 0.5-1.5L/min, and the heating rate of sintering is 5 DEG C/min, first in 525 DEG C of heat preservation 3.5h, then is warming up to 840
DEG C heat preservation 13h, the nickel-cobalt-manganese ternary material of black is obtained after calcining；
(3) nickel-cobalt-manganese ternary material is placed in clear AlOOH colloidal sol, wherein nickel-cobalt-manganese ternary material and AlOOH colloidal sol
Molar ratio is 1:0.004；Continuing agitating and heating, evaporation drying is placed in kiln and is calcined, and 680 DEG C of calcination temperature, calcining
Time is 7.7h, finally obtains alumina-coated nickel-cobalt-manganternary ternary anode material.
Fig. 1 is the XRD diagram of the alumina-coated nickel-cobalt-manganternary ternary anode material of preparation, as can be seen from Figure 1 not miscellaneous
Peak is the base peak of the nickel-cobalt-manganese ternary material (NCM622) of standard, this is because the covering amount of aluminium oxide is less, so detection
Less than the presence of its diffraction maximum.
Embodiment 2
(1) ammonium hydroxide of 1mol/L is added in a reservoir, is placed in laser heating in 80 DEG C of water-baths and stirs, be then slowly dropped into
0.2mol/L aluminum nitrate solution, generates sediment slowly；It reacts to sediment not when increasing, then citric acid is added thereto
With 0.5mol/L nitric acid solution, hydrolyze sediment slowly, peptization continues to obtain clear AlOOH after stirring aging 10-20h
Colloidal sol；
(2) in molar ratio 1:1.06 by presoma Ni0.6Co0.2Mn0.2(OH)2With LITHIUM BATTERY LiOHH2O mixes ball together
Mill, it is to be mixed to be uniformly placed in alumina ceramic crucible, high temperature sintering is carried out in the case where being connected with compressed air, wherein burning
The gas flow of knot is 0.5-1.5L/min, and the heating rate of sintering is 5 DEG C/min, first in 525 DEG C of heat preservation 3.5h, then is warming up to
840 DEG C of heat preservation 13h obtain the nickel-cobalt-manganese ternary material (referred to as uncoated material) of black after sintering；
(3) nickel-cobalt-manganese ternary material is placed in clear AlOOH colloidal sol, wherein nickel-cobalt-manganese ternary material and AlOOH colloidal sol
Molar ratio is 1:0.006；Continuing agitating and heating, evaporation drying is placed in kiln and is calcined, and 680 DEG C of calcination temperature, calcining
Time is 7.7h, finally obtains alumina-coated nickel-cobalt-manganternary ternary anode material (referred to as cladding material).
Fig. 2 is the SEM figure of alumina-coated nickel-cobalt-manganternary ternary anode material prepared by embodiment 2, can be obvious from Fig. 2
See that material surface is uniformly coated with one layer of Al2O3, illustrate to have achieved the purpose that cladding by the method.Respectively to uncoated material
Expect to carry out pH value detection with cladding, uncoated material and the pH value for coating material are respectively 12.32 and 11.74, illustrate the alkali of cladding material
Property it is weaker, surface residual alkali amount is lower, it may thus be appreciated that can reduce the residual alkali amount of material surface by alumina-coated operation.
Embodiment 3
A kind of lithium ion battery, including shell and it is placed in the intracorporal anode of shell, cathode, diaphragm and electrolyte, diaphragm is located at described
Between anode and cathode, diaphragm is gluing ceramic diaphragm, and cathode is artificial graphite, using the LiPF of 1.0mol/L6/EC+EMC+
The electrolyte of DEC (EC, EMC and DEC volume ratio are 3:5:2), shell is rectangular aluminum hull, wherein just extremely prepared by embodiment 2
Cladding material.Show that the cladding material being prepared using the method for the present invention is applied to the excellent properties that battery has, system to compare
Another standby lithium ion battery, is constituted as above-mentioned battery, but is with uncoated material for anode.Detect above two electricity
The high-temperature expansion rate and normal-temperature circulating performance in pond, as a result as shown in Figure 3 and Figure 4.What " cladding " represented in Fig. 3 and Fig. 4 is cladding
Material is battery made of anode, and what " uncoated " represented is uncoated material as battery made of positive.
The test method of the high-temperature expansion rate of battery are as follows: the battery 0.5C multiplying power after forming and capacity dividing is fully charged, so
It is placed in 60 DEG C of environment and shelves 7d, the change rate that the battery case thickness of front and back is shelved in measurement is high-temperature expansion rate.Fig. 3
For the high-temperature expansion rate comparison diagram of two kinds of batteries prepared by embodiment 3, what the battery number in abscissa indicated is every kind of material
The case where 6 batteries are made, detect this 6 batteries, keeps data more representative.It is made as can be seen from Figure 3 with cladding material of anode
Battery, the high-temperature expansion rate of battery is smaller, illustrate by cladding operation after reduce material surface residual alkali amount, can effectively press down
Side reaction between positive electrode and electrolyte processed makes battery produce gas in cyclic process less, so that expansion rate is smaller, effectively mentions
The high security performance of battery.
Fig. 4 is the normal-temperature circulating performance figure of two kinds of batteries prepared by embodiment 3, is anode system with cladding material as can be seen from Figure 4
At battery, the cycle performance of battery is preferable, and capacity retention ratio is still 99.86% after circulation 150 weeks, and is with uncoated material
Battery made of anode is 96.68%, shows there is good cycle performance manufactured battery after cladding operation.
Embodiment 4
(1) ammonium hydroxide of 1mol/L is added in a reservoir, is placed in laser heating in 80 DEG C of water-baths and stirs, be then slowly dropped into
0.2mol/L aluminum nitrate solution, generates sediment slowly；It reacts to sediment not when increasing, then citric acid is added thereto
With 0.5mol/L nitric acid solution, hydrolyze sediment slowly, peptization continues to obtain clear AlOOH after stirring aging 10-20h
Colloidal sol；
(2) in molar ratio 1:1.06 by presoma Ni0.6Co0.2Mn0.2(OH)2With LITHIUM BATTERY LiOHH2O mixes ball together
Mill, it is to be mixed to be uniformly placed in alumina ceramic crucible, high temperature sintering is carried out in the case where being connected with compressed air, wherein burning
The gas flow of knot is 0.5-1.5L/min, and the heating rate of sintering is 5 DEG C/min, first in 525 DEG C of heat preservation 3.5h, then is warming up to
855 DEG C of heat preservation 13h, obtain the nickel-cobalt-manganese ternary material of black after sintering；
(3) nickel-cobalt-manganese ternary material is placed in clear AlOOH colloidal sol, wherein nickel-cobalt-manganese ternary material and AlOOH colloidal sol
Molar ratio is 1:0.006；Continuing agitating and heating, evaporation drying is placed in kiln and is calcined, and 680 DEG C of calcination temperature, calcining
Time is 7.7h, finally obtains alumina-coated nickel-cobalt-manganternary ternary anode material.
In addition, embodiment proposed in this specification and attached drawing are only preferred implementation for illustration purposes
Example, it is no intended to limit the scope of the invention, therefore understands that can make without departing from the spirit and scope of the present invention
Other equivalent schemes and modification.
Claims (10)
1. a kind of preparation method of alumina-coated nickel-cobalt-manganternary ternary anode material, it is characterised in that: the following steps are included:
(1) ammonium hydroxide is added in a reservoir, is placed in heating stirring in water-bath, instills aluminum nitrate solution and generates sediment, reacts to heavy
When starch is not further added by, citric acid and nitric acid is added, hydrolyzes sediment, peptization obtains AlOOH colloidal sol after aging；
(2) nickel cobalt manganese presoma and lithium source ball milling mixing is uniform, nickel-cobalt-manganese ternary material is obtained after oversintering；
(3) nickel-cobalt-manganese ternary material is placed in AlOOH colloidal sol, continues agitating and heating, is calcined after evaporation drying,
Finally obtain alumina-coated nickel-cobalt-manganternary ternary anode material.
2. a kind of preparation method of alumina-coated nickel-cobalt-manganternary ternary anode material according to claim 1, feature exist
In: the concentration of ammonium hydroxide is 0.5-2mol/L in the step (1), and the temperature of water-bath is 80-100 DEG C, the concentration of aluminum nitrate solution
For 0.2-0.6mol/L, the concentration of nitric acid is 0.5-1mol/L；The molar ratio of aluminum nitrate is 1 in citric acid and aluminum nitrate solution:
1。
3. a kind of preparation method of alumina-coated nickel-cobalt-manganternary ternary anode material according to claim 1, feature exist
In: the time of aging is 10-20h in the step (1).
4. a kind of preparation method of alumina-coated nickel-cobalt-manganternary ternary anode material according to claim 1, feature exist
In: lithium source is selected from least one of the oxide of lithium, hydroxide, carbonate, acetate, oxalates in the step (2).
5. a kind of preparation method of alumina-coated nickel-cobalt-manganternary ternary anode material according to claim 1, feature exist
In: the molar ratio of nickel cobalt manganese presoma and lithium source is 1:(1.02-1.07 in the step (2)).
6. a kind of preparation method of alumina-coated nickel-cobalt-manganternary ternary anode material according to claim 1, feature exist
In: the specific steps being sintered in the step (2) are as follows: be warming up to 500-550 DEG C with 5 DEG C/min of heating rate, keep the temperature 3-5h, so
After be continuously heating to 800-870 DEG C, keep the temperature 10-15h；The atmosphere of sintering is one of oxygen, air, compressed air；Sintering
Gas flow be 0.5-1.5L/min.
7. a kind of preparation method of alumina-coated nickel-cobalt-manganternary ternary anode material according to claim 1, feature exist
In: the molar ratio of nickel-cobalt-manganese ternary material and AlOOH colloidal sol is 1:(0.002-0.006 in the step (3)).
8. a kind of preparation method of alumina-coated nickel-cobalt-manganternary ternary anode material according to claim 1, feature exist
In: the heating rate calcined in the step (3) is 5 DEG C/min, and the temperature of calcining is 600-750 DEG C, and the time of calcining is 5-
10h。
9. alumina-coated nickel-cobalt-manganternary ternary anode material made from a kind of preparation method a method as claimed in any one of claims 1-8.
10. a kind of alumina-coated nickel-cobalt-manganternary ternary anode material as claimed in claim 9 is in preparing lithium ion battery
Using.
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| CN111600023A (en) * | 2020-04-09 | 2020-08-28 | 中南大学 | Titanium dioxide coated nickel-cobalt-manganese ternary cathode material and preparation method and application thereof |
| CN112635740A (en) * | 2020-12-28 | 2021-04-09 | 湖北融通高科先进材料有限公司 | Al (aluminum)2O3Preparation method of coated NCM ternary cathode material |
| CN112794372A (en) * | 2020-12-31 | 2021-05-14 | 南通瑞翔新材料有限公司 | Preparation method of composite coated ternary cathode material |
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| CN114560515A (en) * | 2022-03-25 | 2022-05-31 | 骆驼集团资源循环襄阳有限公司 | Method for preparing aluminum-coated ternary precursor by sol-gel method |
| CN114709391A (en) * | 2022-04-01 | 2022-07-05 | 湖北亿纬动力有限公司 | Positive electrode lithium supplement material, preparation method thereof and lithium ion battery |
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| CN114709391A (en) * | 2022-04-01 | 2022-07-05 | 湖北亿纬动力有限公司 | Positive electrode lithium supplement material, preparation method thereof and lithium ion battery |
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